JP5940025B2 - 高純度のパラタングステン酸アンモニウム四水和物 - Google Patents
高純度のパラタングステン酸アンモニウム四水和物 Download PDFInfo
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- JP5940025B2 JP5940025B2 JP2013143060A JP2013143060A JP5940025B2 JP 5940025 B2 JP5940025 B2 JP 5940025B2 JP 2013143060 A JP2013143060 A JP 2013143060A JP 2013143060 A JP2013143060 A JP 2013143060A JP 5940025 B2 JP5940025 B2 JP 5940025B2
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- Prior art keywords
- apw
- ammonium paratungstate
- tetrahydrate
- tungsten
- decahydrate
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- -1 ammonium paratungstate tetrahydrate Chemical class 0.000 title claims description 25
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims 1
- 229910052782 aluminium Inorganic materials 0.000 claims 1
- 238000000034 method Methods 0.000 description 31
- 239000000047 product Substances 0.000 description 29
- 239000000243 solution Substances 0.000 description 23
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 23
- 229910052721 tungsten Inorganic materials 0.000 description 22
- 239000010937 tungsten Substances 0.000 description 22
- 238000004519 manufacturing process Methods 0.000 description 15
- 150000004691 decahydrates Chemical class 0.000 description 13
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 12
- 238000003756 stirring Methods 0.000 description 12
- 150000004685 tetrahydrates Chemical class 0.000 description 12
- XAYGUHUYDMLJJV-UHFFFAOYSA-Z decaazanium;dioxido(dioxo)tungsten;hydron;trioxotungsten Chemical compound [H+].[H+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O XAYGUHUYDMLJJV-UHFFFAOYSA-Z 0.000 description 11
- 239000012074 organic phase Substances 0.000 description 11
- 239000012071 phase Substances 0.000 description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 11
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- 239000012535 impurity Substances 0.000 description 9
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 8
- 239000008346 aqueous phase Substances 0.000 description 8
- 239000007864 aqueous solution Substances 0.000 description 8
- 239000000126 substance Substances 0.000 description 8
- 239000012452 mother liquor Substances 0.000 description 7
- 229910021529 ammonia Inorganic materials 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 238000002360 preparation method Methods 0.000 description 6
- 239000012141 concentrate Substances 0.000 description 5
- 239000013078 crystal Substances 0.000 description 5
- 238000000113 differential scanning calorimetry Methods 0.000 description 5
- 229910052750 molybdenum Inorganic materials 0.000 description 5
- 239000000725 suspension Substances 0.000 description 5
- 239000000956 alloy Substances 0.000 description 4
- 229910045601 alloy Inorganic materials 0.000 description 4
- 229910052785 arsenic Inorganic materials 0.000 description 4
- 238000002425 crystallisation Methods 0.000 description 4
- 230000008025 crystallization Effects 0.000 description 4
- 238000000605 extraction Methods 0.000 description 4
- 238000000622 liquid--liquid extraction Methods 0.000 description 4
- 229910052698 phosphorus Inorganic materials 0.000 description 4
- 229910052710 silicon Inorganic materials 0.000 description 4
- 238000000638 solvent extraction Methods 0.000 description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 150000001412 amines Chemical class 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 230000029087 digestion Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000001704 evaporation Methods 0.000 description 3
- 230000008020 evaporation Effects 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- 238000000746 purification Methods 0.000 description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 description 3
- 235000011121 sodium hydroxide Nutrition 0.000 description 3
- 239000011343 solid material Substances 0.000 description 3
- 238000005477 sputtering target Methods 0.000 description 3
- 239000007858 starting material Substances 0.000 description 3
- YOFPVMWVLDSWKR-UHFFFAOYSA-N 11-methyl-n-(11-methyldodecyl)dodecan-1-amine Chemical compound CC(C)CCCCCCCCCCNCCCCCCCCCCC(C)C YOFPVMWVLDSWKR-UHFFFAOYSA-N 0.000 description 2
- PLLBRTOLHQQAQQ-UHFFFAOYSA-N 8-methylnonan-1-ol Chemical compound CC(C)CCCCCCCO PLLBRTOLHQQAQQ-UHFFFAOYSA-N 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 2
- 238000005349 anion exchange Methods 0.000 description 2
- 239000007900 aqueous suspension Substances 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 239000011733 molybdenum Substances 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M sodium chloride Inorganic materials [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- HYHCSLBZRBJJCH-UHFFFAOYSA-M sodium hydrosulfide Chemical compound [Na+].[SH-] HYHCSLBZRBJJCH-UHFFFAOYSA-M 0.000 description 2
- XMVONEAAOPAGAO-UHFFFAOYSA-N sodium tungstate Chemical compound [Na+].[Na+].[O-][W]([O-])(=O)=O XMVONEAAOPAGAO-UHFFFAOYSA-N 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 229910052720 vanadium Inorganic materials 0.000 description 2
- 229910000616 Ferromanganese Inorganic materials 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- OYASCWOZHBYIGC-UHFFFAOYSA-N azane;tungsten Chemical compound N.[W] OYASCWOZHBYIGC-UHFFFAOYSA-N 0.000 description 1
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 1
- 229910052601 baryte Inorganic materials 0.000 description 1
- 239000010428 baryte Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000010828 elution Methods 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 239000003456 ion exchange resin Substances 0.000 description 1
- 229920003303 ion-exchange polymer Polymers 0.000 description 1
- DALUDRGQOYMVLD-UHFFFAOYSA-N iron manganese Chemical compound [Mn].[Fe] DALUDRGQOYMVLD-UHFFFAOYSA-N 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 description 1
Images
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G41/00—Compounds of tungsten
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/60—Compounds characterised by their crystallite size
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/88—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by thermal analysis data, e.g. TGA, DTA, DSC
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/54—Particles characterised by their aspect ratio, i.e. the ratio of sizes in the longest to the shortest dimension
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/10—Solid density
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/11—Powder tap density
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Description
加熱可能な200lの攪拌反応器中に、3.5g/l NH3、45.2g/1 W及び50lの脱イオン水を有する100lのアンモニウム及びタングステン含有溶液を装入した。さらに、攪拌下で200kgのAPW十水和物を添加した。引き続いて、該懸濁液を3時間に亘って85℃で、攪拌下で処理した。流動相のNH3−濃度は、NH3:W−物質量比 0.83:1の場合に3.5g/lであった。室温でのpH値は6.9であった。固体材料と水性溶液との質量比は1.14:1であった。処理後に、該懸濁液を濾過し、該生成物を10lのVE−水で洗浄し、かつ引き続いて100℃で乾燥させた。生成物量は190kgであった。これは98.1%の収率に相当する。
加熱可能な200lの攪拌反応器中に、215lのVE−水を装入した。さらに、攪拌下で200kgのAPW十水和物を添加した。引き続いて、該懸濁液を2時間に亘って90℃の攪拌下で処理した。流動相のNH3−濃度は、NH3:W−物質量比0.77:1の場合に2.1g/lであった。室温でのpH値は6.8であった。固体材料と水性溶液との質量比は0.80:1であった。処理後に、該懸濁液を濾過し、該生成物を10lのVE−水で洗浄し、かつ引き続いて100℃で乾燥させた。生成物量は184kgであった。これは95.3%の収率に相当する。第1表において、生成物の算出された分析データを表す。
2.)優秀な中国グレード(Hegdu Tungstend)
3.)Specification Wolfram Bergbau und Huettrngrsellschaft m.b.H.
4.)Osram Sylvania
5.)Fujan Xiamen Tungsten Products Plant
6.)Chinese Production, Jiangxi Province
7.)サンプル:Alloys Plant Kirobgrad, Russland
1)〜6)に関する記述は、TUNGSTEN Properties Chemistry, Technology of Element, Alloys and Chemical Compound (ISBN 0-306-45053-4, 1999), Lassner, Scubert、第210頁に由来する。
この例は、図2中に記載された装置に基づいて、本発明によるAPW四水和物の製造を示す。本発明による方法は、図2中に表された装置の一部で実施した。
Claims (1)
- アルミニウムを0.06ppm、あるいは0.05ppm未満含む、生成物の全量に対して少なくとも99.999%の純度を有する、パラタングステン酸アンモニウム四水和物。
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE102007005287.3 | 2007-02-02 | ||
DE102007005287A DE102007005287B4 (de) | 2007-02-02 | 2007-02-02 | Verfahren zur Herstellung von Ammoniumparawolframattetrahydrat und hochreines Ammoniumparawolframattetrahydrat |
Related Parent Applications (1)
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JP2009547659A Division JP5361739B2 (ja) | 2007-02-02 | 2008-01-29 | パラタングステン酸アンモニウム四水和物及び高純度のパラタングステン酸アンモニウム四水和物を製造する方法 |
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JP2013212985A JP2013212985A (ja) | 2013-10-17 |
JP5940025B2 true JP5940025B2 (ja) | 2016-06-29 |
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JP2009547659A Active JP5361739B2 (ja) | 2007-02-02 | 2008-01-29 | パラタングステン酸アンモニウム四水和物及び高純度のパラタングステン酸アンモニウム四水和物を製造する方法 |
JP2013143060A Active JP5940025B2 (ja) | 2007-02-02 | 2013-07-08 | 高純度のパラタングステン酸アンモニウム四水和物 |
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JP2009547659A Active JP5361739B2 (ja) | 2007-02-02 | 2008-01-29 | パラタングステン酸アンモニウム四水和物及び高純度のパラタングステン酸アンモニウム四水和物を製造する方法 |
Country Status (8)
Country | Link |
---|---|
US (2) | US8168155B2 (ja) |
EP (1) | EP2118018B1 (ja) |
JP (2) | JP5361739B2 (ja) |
CN (2) | CN103030178B (ja) |
DE (1) | DE102007005287B4 (ja) |
ES (1) | ES2745085T3 (ja) |
PT (1) | PT2118018T (ja) |
WO (1) | WO2008092838A1 (ja) |
Families Citing this family (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE102007005286B4 (de) | 2007-02-02 | 2009-08-27 | H.C. Starck Gmbh | Verfahren zur Herstellung von Ammoniumparawolframathydraten und Ammoniumparawolframatdekahydrat |
JP5636142B2 (ja) * | 2009-03-02 | 2014-12-03 | 三菱マテリアル株式会社 | 高純度パラタングステン酸アンモニウムの製造方法 |
JP4797099B2 (ja) | 2009-10-01 | 2011-10-19 | Jx日鉱日石金属株式会社 | 高純度タングステン粉末の製造方法 |
CN105849837B (zh) | 2013-12-27 | 2018-05-04 | 昭和电工株式会社 | 钨电容器用阳极体 |
CN109289940B (zh) * | 2018-10-24 | 2021-03-05 | 赣州海创钨业有限公司 | 一种仲钨酸铵生产用离子交换装置 |
CN111689520B (zh) * | 2020-06-17 | 2023-04-18 | 赣州有色冶金研究所有限公司 | 一种二段真空制备十水合仲钨酸铵的方法 |
CN113816428A (zh) * | 2021-10-26 | 2021-12-21 | 赣州市海龙钨钼有限公司 | 一种制备仲钨酸铵的工艺 |
CN113816429B (zh) * | 2021-11-12 | 2023-04-18 | 江西钨业股份有限公司 | 仲钨酸铵的颗粒粗化方法 |
Family Cites Families (15)
Publication number | Priority date | Publication date | Assignee | Title |
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DE1150962B (de) * | 1959-02-10 | 1963-07-04 | Gen Mills Inc | Verfahren zur Abtrennung von Wolframverbindungen aus waessrigen, wolframhaltigen Loesungen |
DE1244141B (de) | 1962-10-26 | 1967-07-13 | Blair Burwell | Verfahren zur Herstellung von hochreinem Ammoniumparawolframat |
US4092400A (en) * | 1977-04-11 | 1978-05-30 | Engelhard Minerals & Chemicals Corp. | Process for recovering high purity tungsten compositions from wolframite ores |
US4115513A (en) | 1977-08-16 | 1978-09-19 | Westinghouse Electric Corp. | Processing of ammonium paratungstate from tungsten ores |
JPS5761632A (en) * | 1980-10-02 | 1982-04-14 | Toshiba Corp | Production of crude particles of ammonium paratungstenate crystal |
US4450144A (en) * | 1981-01-19 | 1984-05-22 | Amax Inc. | Ammonium hydroxide stripping of tungsten from organic solvents |
US4623534A (en) * | 1985-03-21 | 1986-11-18 | Gte Products Corporation | Method for producing ammonium paratungstate |
JPH0227287B2 (ja) * | 1985-11-07 | 1990-06-15 | Nippon Mining Co | Kojundoparatangusutensananmoniumuketsushonoseizohoho |
JPH07121807B2 (ja) * | 1987-12-25 | 1995-12-25 | 株式会社ジャパンエナジー | 高純度パラタングステン酸アンモニウム結晶の製造方法 |
US4969336A (en) * | 1989-08-04 | 1990-11-13 | Cryo-Cell International, Inc. | Cryogenic storage apparatus, particularly with automatic retrieval |
DE19724183C2 (de) * | 1996-07-05 | 1999-03-25 | Starck H C Gmbh Co Kg | Verfahren zur Herstellung reiner Alkali- und/oder Ammonium-Wolframat-Lösungen |
DE19628816A1 (de) | 1996-07-17 | 1998-01-22 | Sawatzki Viktor | Verfahren zur Herstellung von Parawolframat |
CN1377980A (zh) * | 2002-02-06 | 2002-11-06 | 王旭升 | 一种用高钼钨矿制备高纯仲钨酸铵的方法 |
JP2005126321A (ja) * | 2003-09-30 | 2005-05-19 | Jfe Mineral Co Ltd | タングステン酸アンモニウムの製造方法 |
DE102007005286B4 (de) * | 2007-02-02 | 2009-08-27 | H.C. Starck Gmbh | Verfahren zur Herstellung von Ammoniumparawolframathydraten und Ammoniumparawolframatdekahydrat |
-
2007
- 2007-02-02 DE DE102007005287A patent/DE102007005287B4/de active Active
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2008
- 2008-01-29 ES ES08708317T patent/ES2745085T3/es active Active
- 2008-01-29 CN CN201310009900.8A patent/CN103030178B/zh active Active
- 2008-01-29 EP EP08708317.6A patent/EP2118018B1/de active Active
- 2008-01-29 JP JP2009547659A patent/JP5361739B2/ja active Active
- 2008-01-29 US US12/524,968 patent/US8168155B2/en active Active
- 2008-01-29 CN CN2008800039201A patent/CN101600653B/zh active Active
- 2008-01-29 PT PT08708317T patent/PT2118018T/pt unknown
- 2008-01-29 WO PCT/EP2008/051000 patent/WO2008092838A1/de active Application Filing
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2010
- 2010-11-12 US US12/945,038 patent/US8226923B2/en active Active
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Also Published As
Publication number | Publication date |
---|---|
PT2118018T (pt) | 2019-09-17 |
JP5361739B2 (ja) | 2013-12-04 |
ES2745085T3 (es) | 2020-02-27 |
US20100028250A1 (en) | 2010-02-04 |
DE102007005287B4 (de) | 2009-10-01 |
US20110070148A1 (en) | 2011-03-24 |
EP2118018B1 (de) | 2019-06-26 |
CN103030178B (zh) | 2015-11-18 |
CN101600653B (zh) | 2013-07-17 |
US8168155B2 (en) | 2012-05-01 |
WO2008092838A1 (de) | 2008-08-07 |
US8226923B2 (en) | 2012-07-24 |
CN103030178A (zh) | 2013-04-10 |
JP2010517903A (ja) | 2010-05-27 |
JP2013212985A (ja) | 2013-10-17 |
EP2118018A1 (de) | 2009-11-18 |
DE102007005287A1 (de) | 2008-08-14 |
CN101600653A (zh) | 2009-12-09 |
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